Diethylamine → N-ethylethanaminium 4-{1-[({1-[4-(trifluoromethyl)benzyl]-1H-indol-7-yl}carbonyl)amino]cyclopropyl}benzoate

HRID 1694385ノート

反応式

HRID 1694385 の反応式
[F:1][C:2]([F:35])([F:34])[C:3]1[CH:33]=[CH:32][C:6]([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][C:15]=3[C:17]([NH:19][C:20]3([C:23]4[CH:31]=[CH:30][C:26]([C:27]([OH:29])=[O:28])=[CH:25][CH:24]=4)[CH2:22][CH2:21]3)=[O:18])[CH:10]=[CH:9]2)=[CH:5][CH:4]=1.[CH2:36]([NH:38][CH2:39][CH3:40])[CH3:37].COC(C)(C)C>C(O)C>[F:35][C:2]([F:1])([F:34])[C:3]1[CH:33]=[CH:32][C:6]([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][C:15]=3[C:17]([NH:19][C:20]3([C:23]4[CH:24]=[CH:25][C:26]([C:27]([O-:29])=[O:28])=[CH:30][CH:31]=4)[CH2:21][CH2:22]3)=[O:18])[CH:10]=[CH:9]2)=[CH:5][CH:4]=1.[CH2:36]([NH2+:38][CH2:39][CH3:40])[CH3:37]

参加物

5

反応物 3

HCID 8021DiethylamineHCID 15413tert-Butyl methyl etherHCID 250030754-(1-(1-(4-(trifluoromethyl)benzyl)-1H-indole-7-carboxamido)cyclopropyl)benzoic acid

生成物 1

HCID 67279731N-ethylethanaminium 4-{1-[({1-[4-(trifluoromethyl)benzyl]-1H-indol-7-yl}carbonyl)amino]cyclopropyl}benzoate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4-{1-[({1-[4-(trifluoromethyl)benzyl]-1H-indol-7-yl}carbonyl)amino]cyclopropyl}benzoic acid (13 g, 27.2 mmol) was dissolved in 146 ml ethanol. Diethylamine (3.4 ml, 33 mmol) was added and the mixture was stirred 30 min (formation of precipitate observed). 260 ml of methyl tert-butylether was added and the mixture aged one hour. The solid was collected by filtration, washed with methyl tert-butylether and dried under vacuum at 85° C. for 24 h. 1H NMR 6 Acetone-d6: 8.30 (1H, s), 7.90 (2H, d), 7.80 (1H, d), 7.55 (2H, d), 7.45-7.35 (4H, m), 7.15 (1H, d), 7.00 (2H, d), 6.70 (1H, d), 5.80 (2H, s), 2.60 (4H, q), 1.25-1.20 (2H, m), 1.10-1.05 (8H, m).

後処理

  1. customthe mixture aged one hour
  2. filtrationThe solid was collected by filtration
  3. washwashed with methyl tert-butylether
  4. customdried under vacuum at 85° C. for 24 h

出典と根拠

ORDレコード
ord-99f274b087ce41579f6c2661aa68c990
出典データセット
uspto-grants-2012_04
特許番号
US08158671B2

反応ノート

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